CN109437763B - Microcrack self-repairing cement-based composite material and preparation method thereof - Google Patents
Microcrack self-repairing cement-based composite material and preparation method thereof Download PDFInfo
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Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/04—Portland cements
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/34—Non-shrinking or non-cracking materials
- C04B2111/343—Crack resistant materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
Abstract
The invention provides a microcrack self-repairing cement-based composite material and a preparation method thereof. The method comprises the following steps: dispersing graphene oxide and carbon nano onions in a solution to form a mixed solution; adding cement into the mixed solution and uniformly stirring to form cement slurry; adding a filler into the cement slurry to form a graphene oxide/carbon nano onion cement-based composite material, namely a microcrack self-repairing cement-based composite material, wherein the dosage of the graphene oxide accounts for 0.005-5% of the cement, the dosage of the carbon nano onion accounts for 0.005-5% of the cement, and the dosage of the filler accounts for 200-400% of the cement. The invention can obtain the cement-based composite material with microcrack and a certain self-repairing capability; the cement-based composite material with good mechanical property can be obtained.
Description
Technical Field
The invention relates to the technical field of concrete materials and preparation thereof, in particular to a microcrack self-repairing cement-based composite material taking graphene oxide and carbon nano-onion as additives and a preparation method thereof.
Background
The cement-based composite material is widely applied to production and life as the composite material with the largest worldwide consumption. In practical engineering application, however, the cement-based composite material still faces a series of problems such as freeze thawing, carbonization, erosion, corrosion, cracking and the like, so that the performances of all aspects of the cement-based composite material are obviously reduced. In order to meet the requirements of national infrastructure on high-performance cement composite materials, the development of high-strength and high-performance cement-based composite materials is imperative.
Disclosure of Invention
The present invention aims to address at least one of the above-mentioned deficiencies of the prior art. For example, one of the objects of the present invention is to provide a novel cement-based composite material having crack self-repairing capability and a method for preparing the same.
In order to solve the problems, the inventor researches and obtains the graphene oxide/carbon nano onion cement-based composite material and the preparation method thereof. Specifically, carbon nano-onions (CNO) and Graphene (GO) are two nanoscale allotropes of graphite, which are zero-dimensional particles and two-dimensional thin film structures, respectively. The graphene oxide has high strength and flexibility, and the structure of the graphene oxide is rich in hydroxyl, carboxyl, epoxy and other groups, so that the graphene oxide is often used as a reinforcing additive material to be applied to various matrixes, and the comprehensive performance of the matrix material can be remarkably improved. The carbon nano onion has a bent and closed graphite shell structure, so that the carbon nano onion has unique self-lubricating property, chemical stability and good mechanical property. The inventor finds that the graphene oxide can continuously promote the fibrous growth of cement crystals in the cement curing stage, particularly at the place where microcracks are formed in the curing process, so that the self-repairing capability of the microcracks of the cement mortar in the curing process is improved; the unique self-lubricating property of the carbon nano onion can promote the dispersion of the graphene oxide in the cement composite material, and the good mechanical property of the carbon nano onion can play a good pinning effect in the cement composite material, so that the mechanical property of the cement composite material is improved in cooperation with the graphene oxide.
In view of the above, an aspect of the present invention provides a method for preparing a microcrack self-repairing cement-based composite material, which is characterized by comprising the following steps: dispersing graphene oxide and carbon nano onions in a solution to form a mixed solution; adding cement into the mixed solution and uniformly stirring to form cement slurry; adding a filler into the cement slurry to form a graphene oxide/carbon nano onion cement-based composite material, namely a microcrack self-repairing cement-based composite material, wherein the dosage of the graphene oxide accounts for 0.005-5% of the cement, the dosage of the carbon nano onion accounts for 0.005-5% of the cement, and the dosage of the filler accounts for 200-400% of the cement.
According to another aspect of the invention, the cement-based composite material with the self-repairing microcrack is prepared by the preparation method.
Compared with the prior art, the beneficial effects of the invention comprise one or more of the following: the cement-based composite material with microcracks and a certain self-repairing capability can be obtained; the cement-based composite material with good mechanical property can be obtained.
Drawings
Fig. 1, a and b, show electron micrographs of cross sections of samples of an exemplary embodiment of the present invention and comparative example 1, respectively.
A and b in fig. 2 show electron micrographs of the surface of a test specimen of an exemplary embodiment of the present invention; c and d in fig. 2 show electron micrographs of the surface of the sample of comparative example 1.
Detailed Description
Hereinafter, the microcrack self-healing cement-based composite material and the method for preparing the same according to the present invention will be described in detail with reference to exemplary embodiments.
In an exemplary embodiment of the invention, a method for preparing a microcrack self-repairing cement-based composite material may be comprised of the steps of forming a graphene/carbon nano onion mixed solution, forming a cement slurry, and forming a graphene oxide/carbon nano onion cement-based composite material.
The step of forming the mixed solution of graphene and carbon nano-onions may be performed by uniformly dispersing graphene oxide and carbon nano-onions in a solution such as water, water containing an organic additive, or an organic solvent. The dispersing process can also adopt ultrasonic oscillation, mechanical stirring and other means so as to ensure that the dispersing effect is more uniform. In the mixed solution, the amount of the graphene oxide is 0.005-5% of the cement used in the subsequent step of forming cement slurry, and may be 0.5-2% by weight. The dosage of the carbon nano onion accounts for 0.005-5 percent of the cement used in the subsequent step of forming cement slurry, and can also account for 0.5-2.5 percent. In addition, the dosage ratio of the graphene oxide to the carbon nano onion can be 0.01-10: 1. therefore, the agglomeration degree generated by simply adding the graphene oxide or the carbon nano onion into the cement is favorably reduced, and the quality and the performance of the prepared cement composite material are favorably improved.
In addition, the step of forming the mixed solution of graphene and carbon nano-onion may be performed by one of the following methods: (i) firstly, forming a graphene oxide solution, then adding carbon nano-onions into the graphite oxide solution, and uniformly mixing; (ii) firstly, forming a carbon nano onion solution, then adding graphene oxide into the carbon nano onion solution, and uniformly mixing; (iii) respectively forming a graphene oxide solution and a carbon nano onion solution, and then uniformly mixing the graphene oxide solution and the carbon nano onion solution.
Wherein, the step of forming the graphene oxide solution can be realized by uniformly mixing the graphene oxide in a liquid phase of water and/or an organic solvent. For example, the graphene oxide solution formed may be an aqueous solution of graphene oxide, or an aqueous solution containing an organic additive (e.g., a dispersant), or an organic solution of graphene oxide. The solid content of the graphene oxide solution can be 0.1-20 wt%, and can also be 1-4 wt%. The solid content represents the weight percentage of graphene oxide in the graphene oxide solution. The graphene oxide may be layered graphite having several to several tens of layers (e.g., 3 to 30 layers) and containing an oxygen-containing functional group.
The step of forming the carbon nano onion solution may be performed by uniformly mixing the carbon nano onion in a liquid phase of water and/or an organic solvent. For example, the formed carbon nano onion solution can be an aqueous solution of carbon nano onion, or an aqueous solution containing an organic dispersing agent (for example, polyvinylpyrrolidone (PVP), or an organic solution of carbon nano onion, the solid content of the carbon nano onion solution can be 0.01-5 wt%, or 0.1-2 wt%, and the solid content represents the weight percentage of the carbon nano onion in the carbon nano onion solution.
The step of forming the cement slurry can be realized by adding cement into the graphene/carbon nano onion mixed solution formed in the previous step and uniformly stirring. For example, the water in the cement slurry may comprise 40 to 60 wt% of the cement. For example, the mixing may be performed by a cement paste mixer to more uniformly mix the cement slurry. In addition, one or more of dispersing agents, water reducing agents, defoaming agents and other auxiliaries can be added into the graphene/carbon nano onion mixed solution during or before and after the cement is added into the graphene/carbon nano onion mixed solution. For example, the dispersing agent can be PEG series, SDBS series, PVP series and the like, and the adding amount of the dispersing agent can account for 0.01-2% of the using amount of the cement; the water reducing agent can be lignosulphonate, naphthalene, melamine, sulfamate, aliphatic, polycarboxylic acid water reducing agent and the like, and the addition amount of the water reducing agent can account for 0.01-2% of the using amount of the cement; the defoaming agent can be organic silicon defoaming agent, mineral oil defoaming agent, polyether defoaming agent and fatty alcohol defoaming agent, and the addition amount of the defoaming agent can be 0.1% -3% of the cement dosage.
And then, adding a filler into the cement slurry to form the graphene oxide/carbon nano onion cement-based composite material. The cement-based composite material is basically in a slurry state and can be used for pouring various foundation materials or engineering materials needing concrete construction. For example, the filler may be present in an amount of 200% to 400% of the amount of cement used in the step of forming the cement slurry, and may be present in an amount of 250% to 300%. The filler may be a material such as sand and/or slag that can be used in cement construction.
In another exemplary embodiment of the present invention, the method for preparing the graphene oxide/carbon nano onion cement-based composite material may further include a step of aging, setting and curing the cement-based composite material to form a solid graphene oxide/carbon nano onion cement-based composite material. For example, the unset cement-based composite material can be led into a mold to be aged and coagulated at room temperature, a preservative film is covered, after the cement is solidified, the mold is removed and placed in water for curing, and finally the solid graphene oxide/carbon nano onion-based composite material is formed.
Exemplary embodiments of the present invention will be further described below with reference to specific examples.
Example 1
In this example, the amount of cement used was 450 parts by weight, and each weight percentage (wt%) was a percentage relative to the amount of cement used, except for the solid content.
0.1 wt% of Carbon Nano Onion (CNO) and 0.05 wt% of polyvinylpyrrolidone (PVP dispersing agent) are weighed, 135 parts by weight of water is added, and ultrasonic treatment is carried out for 0.5h after stirring for 10 min. Subsequently, 90 parts by weight of an aqueous graphene oxide solution (solid content of 0.5 wt%) was added, and sonication was continued for 1.5 h.
Putting the standard PO42.5 cement and the solution after ultrasonic treatment into a cement paste mixer, mixing and stirring for 0.5 h; adding 1350 parts by weight of standard sand, and continuously stirring for 0.5 h; then pouring the mixture into a mould for aging and condensation at room temperature, and covering a preservative film.
After cement is cured, the mold is dismantled and placed in water for curing, and a cured graphene oxide/carbon nano onion cement-based composite material sample is obtained, namely the microcrack self-repairing cement-based composite material sample can be called as a GO/CNO sample.
Example 2
In this example, the amount of cement used was 450 parts by weight, and each weight percentage (wt%) was a percentage relative to the amount of cement used, except for the solid content.
0.5 wt% of Carbon Nano Onion (CNO) and 0.1 wt% of polyvinylpyrrolidone (PVP dispersing agent) are weighed, 120 parts by weight of water is added, and ultrasonic treatment is carried out for 0.5h after stirring for 20 min. Subsequently, 100 parts by weight of an aqueous graphene oxide solution (solid content of 0.4 wt%) was added, and sonication was continued for 2 hours.
Placing the solution after ultrasonic treatment in a cement paste mixer, and mixing and stirring for 1 h; adding 1350 parts by weight of standard sand, and continuously stirring for 1 hour; then pouring the mixture into a mould for aging and condensation at room temperature, and covering a preservative film. After 24h, the removed mould was placed in a standard curing box for curing for 20 days.
The compressive strength and the flexural strength of the microcrack self-repairing cement-based composite material sample of the example 1 after curing for 3 days and 28 days are shown in table 1, the electron micrograph of the cross section of the sample after curing for 28 days is shown as a in fig. 1, and the electron micrograph of the surface of the sample after curing for 28 days is shown as a and b in fig. 2.
Comparative example 1
450 parts by weight of standard PO42.5 cement was added to 225 parts by weight of water and stirred in a cement paste mixer for 0.5 h. 1350 parts by weight of standard sand were added and stirred in a cement mortar stirrer for 1 hour.
Pouring into a mould, ageing and condensing at room temperature, and covering with a preservative film. After the cement is solidified, the mould is dismantled and placed in water for curing for 3 days and 28 days respectively to obtain the solidified cement.
The compressive strength and flexural strength data of the set cement obtained in this comparative example after 3 days and 28 days of curing are shown in Table 1, the electron micrograph of the cross section thereof after 28 days of curing is shown in b of FIG. 1, and the electron micrographs of the surface thereof after 28 days of curing are shown in c and d of FIG. 2.
As shown in table 1, by comparing the compressive strength data and the flexural strength data of the samples of example 1 and comparative example 1, it can be seen that the graphene oxide/carbon nano onion cement-based composite material of the present invention can significantly improve the mechanical properties of the cement composite material, such as the flexural strength and the tensile strength. For example, for the graphene oxide/carbon nano onion cement-based composite material, the cement composite material can be remarkably improved, the tensile strength can reach more than 34MPa, and the breaking strength can reach more than 6.5MPa after three days of curing; after curing for more than twenty days, the tensile strength can reach more than 62MPa, and the breaking strength can reach more than 8.6 MPa.
TABLE 1 compressive and flexural Strength data for samples of example 3 and comparative examples 1-2
Fig. 1, a and b, show electron micrographs of cross sections of samples of an exemplary embodiment of the present invention and comparative example 1, respectively. It can be seen that a in fig. 1 generates a large amount of fibrous fine crystals, while b in fig. 1 generates coarse, irregular and uneven crystals, which further illustrates that the added additive components in the GO/CNO sample can promote the formation of a more compact and uniform structure of the bonded crystals, which is also beneficial to improving the comprehensive mechanical properties of the material.
A and b in fig. 2 show electron micrographs of the surface of a test specimen of an exemplary embodiment of the present invention; c and d in fig. 2 show electron micrographs of the surface of the sample of comparative example 1. It is obvious from the pictures of a and b in fig. 2 that a large amount of fibrous crystals are generated at the positions where cracks may occur in the GO/CNO sample, and the crystals interpenetrate and grow in the cracks, so that on one hand, the cracks are filled and repaired to prevent the further growth of the cracks, and on the other hand, the concrete on the two sides of the cracks is combined more firmly, thereby improving the comprehensive performance of the material. In contrast, as can be seen from the graphs c and d in fig. 2, the cracks of the sample of comparative example 1 are clearly visible, the cracks are not filled, and first break during later growth or under stress, reducing the material properties.
In the method, the carbon nano onions with self-lubricating property are added into the cement-based composite material in a matching manner, so that the agglomeration of graphene can be reduced, and the dispersibility of graphene oxide in the composite material is promoted; meanwhile, due to the large specific surface area and the multiple functional groups of graphene oxide, regular fibrous crystals (shown as a in fig. 1) are promoted to be generated in the cement-based material; furthermore, the addition of the graphene oxide/carbon nano onion promotes the self-repairing capability of microcracks of the cement-based composite material, and fewer, narrower and even unobvious cracks (as shown in a and b in fig. 2) are formed on the surface and the section, so that the cement-based composite material with more excellent mechanical properties is formed. In addition, the microcrack self-repairing cement-based composite material prepared by the invention also has excellent mechanical properties, such as excellent tensile strength, compressive strength and fracture resistance.
Although the present invention has been described above in connection with the exemplary embodiments and the accompanying drawings, it will be apparent to those of ordinary skill in the art that various modifications may be made to the above-described embodiments without departing from the spirit and scope of the claims.
Claims (8)
1. A preparation method of a microcrack self-repairing cement-based composite material is characterized by comprising the following steps:
dispersing graphene oxide and carbon nano onions in a solution to form a mixed solution;
adding cement into the mixed solution and uniformly stirring to form cement slurry;
adding a filler into the cement slurry to form a graphene oxide/carbon nano onion cement-based composite material, namely a microcrack self-repairing cement-based composite material, wherein the dosage of the graphene oxide accounts for 0.005-5% of the cement, the dosage of the carbon nano onion accounts for 0.005-5% of the cement, and the dosage of the filler accounts for 200-400% of the cement.
2. The method of claim 1, further comprising aging setting and curing the cementitious composite to form a solid graphene oxide/carbon nano onion cementitious composite.
3. The method according to claim 1, wherein the step of forming the mixed solution is performed by adding the graphene oxide solution to the carbon nano onion solution and mixing uniformly.
4. The method of claim 1, wherein the step of forming the cement slurry further comprises adding one or more of a dispersant, a water reducer, and a defoamer to the mixed liquor.
5. The method of claim 1, wherein the filler comprises sand and/or slag.
6. The preparation method of claim 1, wherein the graphene oxide accounts for 0.05-2.0% of the cement, and the carbon nano-onions account for 0.5-2.0% of the cement.
7. The method of claim 1, wherein the filler is used in an amount of 250% to 330% of the cement.
8. A microcrack self-repairing cement-based composite material, wherein the cement-based composite material is obtained by the preparation method according to any one of claims 1 to 7.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103130436A (en) * | 2013-03-25 | 2013-06-05 | 中国科学院上海硅酸盐研究所 | Oxidized graphene and graphene reinforced cement based composite material and preparation method thereof |
| CN106191804A (en) * | 2016-06-06 | 2016-12-07 | 重庆大学 | A kind of preparation method of magnetic graphene nano belt/graphene composite film |
| US9862602B1 (en) * | 2017-03-27 | 2018-01-09 | Lyten, Inc. | Cracking of a process gas |
| CN108892407A (en) * | 2018-07-27 | 2018-11-27 | 安徽工业大学 | A kind of bivalve layer epoxy resin micro-capsule self-repair material and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103130436A (en) * | 2013-03-25 | 2013-06-05 | 中国科学院上海硅酸盐研究所 | Oxidized graphene and graphene reinforced cement based composite material and preparation method thereof |
| CN106191804A (en) * | 2016-06-06 | 2016-12-07 | 重庆大学 | A kind of preparation method of magnetic graphene nano belt/graphene composite film |
| US9862602B1 (en) * | 2017-03-27 | 2018-01-09 | Lyten, Inc. | Cracking of a process gas |
| CN108892407A (en) * | 2018-07-27 | 2018-11-27 | 安徽工业大学 | A kind of bivalve layer epoxy resin micro-capsule self-repair material and preparation method thereof |
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